CN102899636B - A kind of method of In-Situ Cleaning MOCVD reaction chamber - Google Patents
A kind of method of In-Situ Cleaning MOCVD reaction chamber Download PDFInfo
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- CN102899636B CN102899636B CN201210364958.XA CN201210364958A CN102899636B CN 102899636 B CN102899636 B CN 102899636B CN 201210364958 A CN201210364958 A CN 201210364958A CN 102899636 B CN102899636 B CN 102899636B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
- H01J37/32853—Hygiene
- H01J37/32862—In situ cleaning of vessels and/or internal parts
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Abstract
The embodiment of the present invention provides a kind of method of In-Situ Cleaning MOCVD reaction chamber, described method comprises: pass into the first clean air to described reaction chamber inside, and by described first clean air at described reaction chamber Internal reforming be the first cleaning plasma to remove the carbonaceous organic material of described reaction chamber inside completely, wherein this first clean air comprises the first oxygen-containing gas; Pass into the second clean air to described reaction chamber inside, and by Internal reforming at described reaction chamber for described second clean air be that the second cleaning plasma is to remove the metal oxide of described reaction chamber inside completely; Wherein said second clean air comprises the first halogen-containing gas.The method of the In-Situ Cleaning MOCVD reaction chamber that the embodiment of the present invention provides has good cleaning effect for the settling on the relatively low surface of reaction chamber internal temperature.
Description
Technical field
The present invention relates to technical field of manufacturing semiconductors, be specifically related to a kind of method of In-Situ Cleaning MOCVD reaction chamber.
Background technology
At present, MOCVD (Metal-organicChemicalVaporDeposition, MOCVD) technology is widely used in the compound (as GaN, InN, AlN, InGaN, AlGaN, GaP etc.) preparing group III element and group Ⅴ element.In the state of the art, prepare after a subject matter that MOCVD reaction chamber after the compound of group III element and group Ⅴ element exists is each reactions steps and can form unnecessary solid by-product settling (as carbonaceous organic material or metal and compound etc. thereof) in reaction chamber inside, these deposits in reaction chamber inside (as spray header, the place such as pedestal and inwall), cause process deviation (processdrift), degradation, and easily in the process of compound preparing group III element and group Ⅴ element, form the impurity such as particle at substrate surface, these impurity can affect subsequent technique, therefore, in use, need to clean the reaction chamber of MOCVD, to remove the settling of reaction chamber inside, and then improve the quality preparing the compound of group III element and group Ⅴ element.
In prior art, the settling removing MOCVD reaction chamber inside generally adopts the mode manually removed, and namely opens MOCVD reaction chamber, then manually removes the settling at the first-class place of spray.But, adopt that this cleaning method productivity is low, repeatability is poor, cleaning efficiency is not high.For this reason, have some to adopt original position to remove the method for MOCVD reaction chamber inside deposition thing in prior art, it is inner to carry out original position removal to settling that the gas containing halogenide (halidechemistries) (as Cl2, HCl, HBr etc.) is mainly passed into MOCVD reaction chamber by these methods.This cleaning method without the need to opening MOCVD reaction chamber, favorable repeatability, cleaning efficiency is high, productivity is high.
But, on the surface (as adopted spray header surface or the reaction chamber inner wall surface of water-cooled) that temperature is relatively low, due to the incomplete decomposing of organometallics forerunner reactant (precursors), these unnecessary settlings mainly comprise polymkeric substance and metal and the compound thereof of metastable organism ligand (organicligands) or association usually, the wherein carbonaceous organic material of the polymkeric substance mainly high density of these metastable organism ligands (organicligands) or association, now, this based on simple halogenide (as Cl
2, HCl, HBr etc.) In-Situ Cleaning method inoperative to removing the settling on the relatively low surface of temperature.
Summary of the invention
For removing the settling on the relatively low surface of MOCVD reaction chamber internal temperature, the embodiment of the present invention provides a kind of method of In-Situ Cleaning MOCVD reaction chamber inside deposition thing, and described method comprises:
Perform step (a):
Pass into the first clean air to described reaction chamber inside, and by Internal reforming at described reaction chamber for described first clean air be the first cleaning plasma; And/or,
In described reaction chamber outside, described first clean air is converted into described first cleaning plasma, and it is inner described first cleaning plasma to be passed into described reaction chamber; And/or,
Pass into described first clean air to described reaction chamber inside, and the temperature maintaining described reaction chamber inside is between 200 DEG C to 500 DEG C;
And the pressure of described reaction chamber inside is remained on first time period in the first predetermined pressure range with remove completely described reaction chamber inside carbonaceous organic material and by the metal of described reaction chamber inside and converting compounds thereof for metal oxide; Wherein, described first clean air comprises the first oxygen-containing gas;
Perform step (b):
Pass into the second clean air to described reaction chamber inside, and by Internal reforming at described reaction chamber for described second clean air be the second cleaning plasma; And/or,
In described reaction chamber outside, described second clean air is converted into described second cleaning plasma, and it is inner described second cleaning plasma to be passed into described reaction chamber; And/or,
Pass into described second clean air to described reaction chamber inside, and the temperature maintaining described reaction chamber inside is between 200 DEG C to 500 DEG C;
And the pressure of described reaction chamber inside to be remained in the second predetermined pressure range for the second time period to remove the metal oxide of described reaction chamber inside completely; Wherein said second clean air comprises the first halogen-containing gas.
Preferably, described first clean air also comprises Ar; And/or described second clean air also comprises Ar.
Preferably, described first clean air also comprises the second halogen-containing gas, and described second halogen-containing gas comprises HCl, BCl
3, Cl
2, H
2/ Cl
2mixed gas, one or several combination in HBr.
Preferably, described in described first clean air, the molar fraction of the first oxygen-containing gas is greater than the molar fraction of described second halogen-containing gas.
Preferably, described second clean air also comprises the second oxygen-containing gas, and described second oxygen-containing gas comprises O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O, CO.
Preferably, described in described second clean air, the molar fraction of the first halogen-containing gas is greater than the molar fraction of described second oxygen-containing gas.
Preferably, described first oxygen-containing gas comprises O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O.
Preferably, described first halogen-containing gas comprises HCl, BCl3, BCl/O
2mixed gas, H
2/ Cl
2mixed gas, Cl
2, one or several combination in HBr.
Preferably, described first time period is greater than 5 minutes, and described second time period is greater than 3 minutes.
In the embodiment of the present invention, the carbonaceous organic material adopting the first clean air and/or its plasma body removal reaction chamber inside comprising the first oxygen-containing gas, the metal adopting the second clean air and/or its plasma body removal reaction chamber inside comprising the first halogen-containing gas and compound thereof.The method of the In-Situ Cleaning MOCVD reaction chamber that the embodiment of the present invention provides can remove polymkeric substance containing metastable organism ligand or association and metal and compound thereof, thus has good cleaning effect for the settling on the relatively low surface of reaction chamber internal temperature.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, mark identical in figure represents identical parts, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.Reference numeral identical in whole accompanying drawing indicates identical part.Deliberately do not draw accompanying drawing by physical size equal proportion convergent-divergent, focus on purport of the present invention is shown.
Fig. 1 is the method flow diagram of the In-Situ Cleaning MOCVD reaction chamber of the embodiment of the present invention one;
Fig. 2 is the structural representation of the MOCVD reaction chamber of the embodiment of the present invention;
Fig. 3 is the method flow diagram of the In-Situ Cleaning MOCVD reaction chamber of the embodiment of the present invention two;
Fig. 4 is the method flow diagram of the In-Situ Cleaning MOCVD reaction chamber of the embodiment of the present invention three.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
For solving the problem removing the sedimental DeGrain on the relatively low surface of MOCVD reaction chamber internal temperature in prior art, present inventor is through having researched and proposed a kind of method of In-Situ Cleaning MOCVD reaction chamber.Below the method for this In-Situ Cleaning MOCVD reaction chamber is described in detail.
Embodiment one
As shown in Figure 1, the schema of the method for the In-Situ Cleaning MOCVD reaction chamber of the embodiment of the present invention one, the structural representation (i.e. Fig. 2) below in conjunction with MOCVD reaction chamber is described in detail to the method.
Step S101: pass into the first clean air to reaction chamber 10 inside, by Internal reforming at reaction chamber 10 for the first clean air be the first cleaning plasma, and the pressure of reaction chamber 10 inside is remained on first time period in the first predetermined pressure range with remove reaction chamber 10 inside carbonaceous organic material and by the convert metals of reaction chamber 10 inside for metal oxide;
Particularly, the first clean air in the embodiment of the present invention one can comprise the first oxygen-containing gas, and wherein the first oxygen-containing gas can be O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O; Preferably, the first oxygen-containing gas in the embodiment of the present invention selects the gas with strong oxidizing property, as O
3, H
2o
2deng.
If the first clean air only comprises a kind of gas, then by an intake ducting (such as intake ducting 41 or 42), this gas can be passed into reaction chamber 10 inside; If the first clean air comprises multiple gases, then by many intake ductings, this multiple gases can be passed into reaction chamber 10 inside, to ensure that these gases pass into reaction chamber 10 respectively, namely these gases just mix after entering reaction chamber 10 inside; In addition, if the first clean air comprises multiple gases, then these gases also can mix before passing into reaction chamber 10 inside, then the gas after this mixing were passed into reaction chamber 10 by intake ducting 41 or 42 inner.
The first clean air in this step S101 is converted into plasma body after entering reaction chamber 10 inside.Particularly, the radio-frequency voltage of certain power can be applied between the spray header 11 of reaction chamber 10 inside and pedestal 13, can be the region between spray header 11 and pedestal 13 by this radio-frequency voltage reaction zone M(such as this reaction zone in reaction chamber 10 inside, substrate used when wherein pedestal 13 is for laying the compound preparing group III element and group Ⅴ element) the first clean air is converted into the first cleaning plasma; In addition, also the region outside the reaction zone of reaction chamber 10 inside the first clean air can be converted into the first cleaning plasma: specifically can apply the radio-frequency voltage of certain power or between reaction chamber 10 inwall and spray header 11, apply the radio-frequency voltage of certain power between reaction chamber 10 inwall and pedestal 13, by the region of this radio-frequency voltage beyond the M of reaction zone (in Fig. 2 the inner region except the M of region of reaction chamber 10), the first clean air be converted into the first cleaning plasma.Certainly, the mode in the embodiment of the present invention one, first clean air being converted into plasma body is not limited to these two kinds, other conventional modes of this area can also be adopted to carry out, do not repeat them here.
First clean air reaction chamber 10 is Internal reforming be the first cleaning plasma after, the pressure first time period (being such as greater than 5 minutes) in the first predetermined pressure (such as 0.1 ~ 10 holder) scope maintaining reaction chamber inside is fully carried out to make the first step cleaning (namely removing the step of the carbonaceous organic material of reaction chamber inside), and the pressure that such as can maintain reaction chamber inside keeps 5 ~ 30 minutes in 0.1 ~ 1 holder scope.Those skilled in the art can select suitable reaction chamber pressure and reaction times when actual requirement for cleaning, do not enumerate at this.
In cleaning course, gas barrier 12 can be kept to be in opened condition always, gaseous product after the settling of the first cleaning plasma and reaction chamber 10 inside can being reacted on the one hand constantly discharges reaction chamber with the carrying out of expedite clean-up process with improve cleaning effect, reaction chamber 10 inside can also be kept to have certain pressure to meet the needs of cleaning course on the other hand, namely, the pressure of reaction chamber 10 inside can also be controlled by the opening degree controlling gas barrier 12 in the embodiment of the present invention one, namely the free air delivery by controlling gas barrier 12 controls the pressure of reaction chamber 10 inside.
In this step, mainly utilize the first oxygen-containing gas (O
2, H
2o
2deng) oxidation susceptibility the carbonaceous organic material in the settling of reaction chamber inside is converted into the hydrocarbon of gaseous state thus discharges reaction chamber 10 by gas barrier 12, and then remove the organism of reaction chamber 10 inside.In addition, the part metals in the settling of reaction chamber 10 inside and compound oxidation thereof can also be become metal oxide by oxygen-containing gas, and these metal oxide ratios are easier to remove in subsequent step.
In addition, settling in view of reaction chamber 10 inside is generally that carbonaceous organic material is together with metal and compound thereof, when settling is thicker, only adopt first clean air with oxidation susceptibility possibly carbonaceous organic materials whole in settling cannot be converted into the carbon compound of gaseous state, this is because the carbonaceous organic material of settling bottom is covered by the metal on its upper strata and compound thereof, therefore, fully react to make the carbonaceous organic material in settling, a certain amount of second halogen-containing gas can also be contained in first clean air in this step, now, easily react with the second halogen-containing gas metal halide of metal halide this gaseous state simultaneously generating gaseous state of the metal on carbonaceous organic material upper strata and compound thereof can discharge reaction chamber 10 by gas barrier 12.Such as, MOCVD reaction chamber is inner easily remains metal and the compounds thereof such as GaN, InN, AlN, the second halogen-containing gas (such as Cl of reaction chamber 10 inside usually
2) plasma body can react with the metal such as GaN, InN, AlN and compound thereof, generate the GaCl of gaseous state
3, InCl
3, AlCl
3deng.
Main purpose in view of this step S101 removes the carbonaceous organic material of reaction chamber inside, therefore, the molar fraction of the oxygen-containing gas in this step in the first clean air can be greater than the molar fraction of the second halogen-containing gas, and wherein the second halogen-containing gas can comprise HCl, BCl
3, Cl
2, H
2/ Cl
2mixed gas, one or several combination in HBr (" H in the application
2/ Cl
2mixed gas " expression " H
2with Cl
2mixed gas ", other similar descriptions represent similar implication).Certainly this is a preferred mode, and the ratio of the molar fraction of the reducing gas in fact in the first clean air and the molar fraction of the second halogen-containing gas can be unrestricted.
In addition, for improving cleaning effect and cleaning speed, the first clean air in this step can also comprise a certain amount of Ar, Ar can be converted into Ar plasma body in reaction chamber 10 inside, and Ar plasma body can the carrying out of expedite clean-up reaction (comprise reducing gas and carbonaceous organic material reacts and/or halogen-containing gas and metal and compound thereof react).
The plasma body be transformed by the first clean air is under the conditions such as suitable temperature and pressure, the carbon bonds of carbonaceous organic material or polymkeric substance can be made, react and generate the carbon compound of gaseous state, thus make the inner metastable organism ligand of reaction chamber and polymer transition be the material of active higher easy removal, these materials can be pumped from reaction chamber with air-flow under the conditions such as particular airflow, pressure, temperature, thus reach clean object.
It should be noted that, in the embodiment of the present invention one, any one in following step S101-A1 and step S101-A2 or two steps can be performed, with alternative steps S101:
Step S101-A1: the first clean air is converted into the first cleaning plasma in reaction chamber 10 outside, and it is inner the first cleaning plasma to be passed into reaction chamber 10;
Step S101-A2: pass into the first clean air to reaction chamber 10 inside, and the temperature maintaining reaction chamber 10 inside is between 200 DEG C to 500 DEG C;
Wherein, the first clean air in step S101-A1 and step S101-A2 can have identical implication with the first clean air in step S101, this place " has identical implication " and refers to that first clean air at this place and the first clean air in step S101 have identical scope (as all comprised the first oxygen-containing gas), but, can select different types of gas within the scope of this, the description of " having identical implication " in following content is with similar herein.
In addition, step S101-A1 and step S101-A2 can also be performed while execution step S101, with the speed of this further expedite clean-up reaction.
Step S102: pass into the second clean air to reaction chamber 10 inside, by Internal reforming at reaction chamber 10 for the second clean air be the second cleaning plasma, and the pressure of reaction chamber 10 inside to be remained in the second predetermined pressure range for the second time period to remove metal and the compound thereof of reaction chamber 10 inside;
The second clean air in the embodiment of the present invention one can comprise the first halogen-containing gas, and this first halogen-containing gas can be HCl, BCl
3, Cl
2, H
2/ Cl
2mixed gas, one or several combination in HBr.
Particularly, the second clean air can be passed into by intake ducting 41 or 42 to reaction chamber 10 inside.Through step S101, the carbonaceous organic material of reaction chamber 10 inside is substantially eliminated, remaining mainly metal (such as Ga, Al, In etc.) and compound, therefore, pass into the second clean air comprising halogen-containing gas to reaction chamber 10 inside in this step, this second clean air can the regioinvertions under the effect of radio-frequency voltage outside the reaction zone M of reaction chamber inside or reaction zone M be plasma body (description see in step S101), this plasma body can fully react with remaining metal in settling and compound thereof the metal halide being formed as gaseous state, the metal halide of these gaseous states discharges reaction chamber 10 by gas barrier 12 subsequently.
Second clean air reaction chamber 10 is Internal reforming be plasma body after, pressure second time period (being such as greater than 3 minutes) in the second predetermined pressure (as 0.1 ~ 10 holder) scope maintaining reaction chamber inside fully carries out to make second step cleaning (namely removing metal and the compound thereof of reaction chamber inside), to remove metal in reaction chamber and compound residues thereof completely, such as can by the maintenance 5 ~ 30 minutes in 0.1 ~ 1 holder scope of the pressure of reaction chamber.Those skilled in the art can select pressure and the reaction times of suitable reaction chamber inside when actual requirement for cleaning, do not enumerate at this.In addition, a small amount of metal oxide produced in step S101 can also be removed in this step.
Particularly, the pressure of reaction chamber 10 inside can be controlled by the flow controlling to pass into the second clean air of reaction chamber 10, or also can be controlled the pressure of reaction chamber 10 inside by the opening degree controlling gas barrier 12.
In this step, main utilization is converted into the reactive metal oxide produced in the halogen of plasma body and the residual metal of reaction chamber inside and compound thereof and step S101, thus the metal halide being gaseous state by these residual metals and compound thereof and convert metal oxides discharges reaction chamber 10.Such as, MOCVD reaction chamber is inner easily remains metal and the compounds thereof such as Ga, In, Al, GaN, InN, AlN, the second halogen-containing gas (such as Cl of reaction chamber 10 inside usually
2) plasma body can react with the metal such as Ga, In, Al, GaN, InN, AlN and compound thereof, generate the GaCl of gaseous state
3, InCl
3, AlCl
3deng.
In addition, can also containing a certain amount of second oxygen-containing gas (as O in the second clean air in this step S102
2), this second oxygen-containing gas can Internal reforming at reaction chamber 10 be plasma body, then react with the carbonaceous organic material that may remain in reaction chamber 10 inside, all to remove the carbonaceous organic material in settling, improve cleaning effect further.
Main purpose in view of this step S102 removes the metal of reaction chamber inside and compound thereof and a small amount of metal oxide, therefore, the molar fraction of the first halogen-containing gas in this step in the second clean air can be greater than the molar fraction of the second oxygen-containing gas, certainly this is a preferred mode, and the ratio of the molar fraction of the first halogen-containing gas in fact in the second clean air and the molar fraction of the second oxygen-containing gas can be unrestricted.
Meanwhile, for improving cleaning effect and cleaning speed further, in this step, can also comprise appropriate Ar in the second clean air, Ar is Internal reforming at reaction chamber 10 is Ar plasma body, and Ar plasma body can the carrying out of accelerated reaction.
It should be noted that, in the embodiment of the present invention one, any one in following step S102-B1 and step S102-B2 or two steps can be performed, with alternative steps S102:
Step S102-B1: the second clean air is converted into the second cleaning plasma in reaction chamber 10 outside, and it is inner the second cleaning plasma to be passed into reaction chamber 10;
Step S102-B2: pass into the second clean air to reaction chamber 10 inside, and the temperature maintaining reaction chamber 10 inside is between 200 DEG C to 500 DEG C;
Wherein, the second clean air in step S102-B1 and step S102-B2 can have identical implication with the second clean air in step S102.
In addition, step S102-A1 and step S102-A2 can also be performed while execution step S102, with the speed of this further expedite clean-up reaction.
The method of the In-Situ Cleaning MOCVD reaction chamber that the embodiment of the present invention one provides, first pass into reaction chamber inside the first clean air comprising the first oxygen-containing gas, in reaction chamber inside, the first clean air be converted into plasma body and utilize its oxidation susceptibility to remove the carbonaceous organic material of reaction chamber inside; Then pass into reaction chamber inside the second clean air comprising the first halogen-containing gas, be used for removing the residual metal of reaction chamber inside and compound thereof and a small amount of metal oxide at the inner plasma body that to be converted into by second clean air of reaction chamber, thus remove the settling of MOCVD reaction chamber inside completely.
It should be noted that, in the embodiment of the present invention one, the execution of step S101 and step S102 can continuous print, namely performs step S102 immediately after execution of step S101; The execution of step S101 and step S102 also can be interval, namely step S102 is performed again every for some time after execution of step S101, certainly, have a rest here in process, gas barrier 12 can be kept to be in exhaust condition always, the gaseous product produced in step S101 all can be discharged reaction chamber like this, and then the cleaning efficiency of step S102 can be improved.
It should be noted that, in the embodiment of the present invention one, can time of performing of proper extension step S101 and/or step S102, to be removed the carbonaceous organic material of reaction chamber inside by step S101 completely, to be removed metal and the compound thereof of reaction chamber inside by step S102 completely, those skilled in the art can adopt the carbonaceous organic material of auxiliary test set monitoring reaction chamber inside and/or metal and compound thereof to be completely removed, in view of the emphasis that this content is not the application, be not described in detail in this.
In addition, also can be cycled to repeat in the embodiment of the present invention and perform step S101 and step S102, to improve cleaning effect further.
Be described in detail with the technical scheme of two concrete examples to the embodiment of the present invention one below:
Example one:
A, simultaneously in reaction chamber 10, pass into O
2, Cl
2and Ar, O can be passed into by the intake ducting shown in Fig. 2 respectively in reaction chamber 10 particularly
2, Cl
2and Ar, O
2, Cl
2250sccm, 250sccm and 500sccm is respectively with the flow of Ar, radio-frequency voltage is added between spray header 11 and reaction chamber 10 inwall, maintenance radio frequency power is 2000W, rf frequency is 13.56MHz, keeps that the pressure of reaction chamber inside is 0.72Torr, the plasma reaction time is 10 minutes (namely first time period is 10 minutes); Through this step, carbonaceous organic materials most in the settling of reaction chamber inside is removed;
B, simultaneously in reaction chamber 10, pass into HCl and Ar, the flow of HCl and Ar is 500sccm, radio-frequency voltage is added between spray header 11 and reaction chamber 10 inwall, maintenance radio frequency power is 2000W, rf frequency is 13.56MHz, keeps that the pressure of reaction chamber inside is 0.68Torr, the plasma reaction time is 5 minutes (namely the second time period was 5 minutes); Through this step, the settling of reaction chamber inside all can be removed.
Example two:
A, simultaneously in reaction chamber 10, pass into O
2, Cl
2and Ar, O can be passed into by the intake ducting shown in Fig. 2 respectively in reaction chamber 10 particularly
2, Cl
2and Ar, O
2, Cl
2250sccm, 250sccm and 500sccm is respectively with the flow of Ar, radio-frequency voltage is added between spray header 11 and reaction chamber 10 inwall, maintenance radio frequency power is 2000W, rf frequency is 13.56MHz, keeps that the pressure of reaction chamber inside is 0.72Torr, the plasma reaction time is 10 minutes; Through this step, the carbonaceous organic material of the overwhelming majority in the settling of reaction chamber inside is removed; In addition, in this step, oxygen-containing gas can also react with the part metals in settling and compound thereof and forms metal oxide;
B, simultaneously in reaction chamber 10, pass into H
2, Cl
2and Ar, H
2, Cl
2250sccm, 250sccm and 500sccm is respectively with the flow of Ar, radio-frequency voltage is added between spray header 11 and reaction chamber 10 inwall, maintenance radio frequency power is 2000W, rf frequency is 13.56MHz, keeps that the pressure of reaction chamber inside is 0.68Torr, the plasma reaction time is 5 minutes; Through this step, carbonaceous organic materials most in the settling of reaction chamber 10 inside and metal and compound thereof and metal oxide all can be removed;
Usually need to pass into H to MOCVD reaction chamber inside in view of when preparing the compound of group III element and group Ⅴ element in MOCVD
2and Cl
2, in this step, material adopts H
2and Cl
2mixed gas remove metal in settling and compound thereof, just without the need to adding extra gas to reaction chamber 10 inside, therefore, not only can simplifying cleaning procedure, the cleaning device (namely without the need to increasing too much intake ducting) of MOCVD reaction chamber can also being simplified.
It should be noted that, in the embodiment of the present invention, clean in the process (as step S101, step S101-A1, step S102, step S102-B1 etc.) of MOCVD reaction chamber in position, can reaction chamber 10 be heated, make reaction chamber 10 inside keep certain temperature.So not only can improve the clean rate of In-Situ Cleaning, can also ensure plasma body and settling react after product be gaseous state, this product is avoided to run into the lower surperficial liquefy of temperature or solid-state and remain in reaction chamber inside, such as can keep the temperature of reaction chamber 10 inside (as 70 DEG C, 80 DEG C or 100 DEG C etc.) between 70 ~ 100 DEG C, the mode heated reaction chamber outer wall or inwall specifically can be adopted to keep the temperature of reaction chamber inside.
The method of the clean MOCVD reaction chamber in the embodiment of the present invention is reacted mainly through the plasma body and settling with reducing property thus changes settling into gaseous product, and by gas barrier, gaseous product is discharged reaction chamber inside.The settling (especially the settling on the surface that temperature is relatively low) that the In-Situ Cleaning method provided by the embodiment of the present invention one removes MOCVD reaction chamber inside can realize process stabilizing, performance boost, and whole MOCVD technique can be made automatically to carry out.
It should be noted that, the In-Situ Cleaning method of the MOCVD reaction chamber that the embodiment of the present invention provides can also adopt other modes.Such as, this cleaning plasma can produce in reaction chamber inside, also can produce in reaction chamber outside and then pass into reaction chamber inside.
Embodiment two
The method of the In-Situ Cleaning MOCVD reaction chamber of the embodiment of the present invention two and the method for the embodiment of the present invention one similar, different is, plasma body in the embodiment of the present invention two can produce in the outside of reaction chamber 10, and then passes into reaction chamber inside by intake ducting.For simplicity, only introduce the difference with the embodiment of the present invention one in the embodiment of the present invention two, those skilled in the art easily obtain the other guide of the embodiment of the present invention two from the associated description of the embodiment of the present invention one, do not repeat them here.
Step S301: the first clean air is converted into the first cleaning plasma in reaction chamber 10 outside, and the first cleaning plasma is passed into the inside of reaction chamber 10, the pressure of reaction chamber 10 inside is remained on first time period in the first predetermined pressure range with remove reaction chamber 10 inside carbonaceous organic material and by part metals and converting compounds thereof for metal oxide;
The first clean air in the embodiment of the present invention two can comprise the first oxygen-containing gas, and wherein the first oxygen-containing gas can be O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O; Preferably, the first oxygen-containing gas in the embodiment of the present invention selects the gas with strong oxidizing property, as O
3, H
2o
2deng.
Particularly, first cleaning plasma can be transformed by using plasma conversion system, such as, first can pass into the first oxygen-containing gas to plasma-converted device inside, then in plasma-converted device inside, the first oxygen-containing gas is converted into the first cleaning plasma.First cleaning plasma can pass into reaction chamber inside by the diffuser be connected with reaction chamber.
After first cleaning plasma passes into reaction chamber inside, maintain reaction chamber pressure first time period in the first predetermined pressure range, the pressure that such as can maintain reaction chamber inside, in 0.1 ~ 10 holder scope (example as the first predetermined pressure range) interior more than 5 minutes (such as 5 ~ 30 minutes), reacts to make the carbonaceous organic material in the first cleaning plasma and settling.
It should be noted that, in the embodiment of the present invention two, any one or two steps in following step S301-A1 and step S301-A2 can be performed with alternative steps S301:
Step S301-A1: pass into the first clean air to reaction chamber 10 inside, and by Internal reforming at reaction chamber 10 for the first clean air be the first cleaning plasma;
Step S301-A2: pass into the first clean air to reaction chamber 10 inside, and the temperature maintaining reaction chamber 10 inside is between 200 DEG C to 500 DEG C;
Wherein, the first clean air in step S301-A1 and step S301-A2 can have identical implication with the first clean air in step S301.
In addition, step S301-A1 and step S301-A2 can also be performed, the speed of reacting with further expedite clean-up while execution step S301.
Step S302: the second clean air is converted into the second cleaning plasma in reaction chamber 10 outside, and it is inner the second cleaning plasma to be passed into reaction chamber 10, the pressure of reaction chamber 10 inside to be remained in the second predetermined pressure range for the second time period to remove metal and the compound thereof of reaction chamber 10 inside;
Particularly, this first cleaning plasma can utilize plasma-converted device to be transformed, such as, first can pass into the first clean air to plasma-converted device inside, then in plasma-converted device inside, the first clean air is converted into the first cleaning plasma.
After second cleaning plasma passes into reaction chamber 10 inside, the pressure of reaction chamber 10 inside can be maintained in the example of 0.1Torr ~ 10Torr(as the second predetermined pressure range) between more than 3 minutes (as 5 ~ 30 minutes), by gas barrier, the metal halide of these gaseous states is discharged reaction chamber with the metal halide making in the second cleaning plasma and settling residual metal and compound thereof fully react to form gaseous state.
The first clean air in the embodiment of the present invention two and the first clean air in the embodiment of the present invention one have the second clean air in identical implication, the embodiment of the present invention two and the second clean air in the embodiment of the present invention one has identical implication.
It should be noted that; parameter (as pressure, time, temperature etc.), gaseous fraction, content etc. in the embodiment of the present invention one describe the scheme be equally applicable in the embodiment of the present invention two; for simplicity; in this no longer repeated description; but the scheme in the embodiment of the present invention two still can combine with the corresponding contents in the embodiment of the present invention one thus obtain concrete implementation by those of ordinary skill in the art, and these implementations are still within protection scope of the present invention.
In the outside of reaction chamber 10, first clean air is converted into the first cleaning plasma in the embodiment of the present invention two, the second clean air is converted into the second cleaning plasma, and the inside the first cleaning plasma being passed into reaction chamber 10 with remove completely reaction chamber 10 inside carbonaceous organic material, the second cleaning plasma is passed into reaction chamber 10 inside to remove metal and the compound thereof of reaction chamber 10 inside completely.
It should be noted that, in the embodiment of the present invention two, the execution of step S301 and step S302 can continuous print, namely performs step S302 immediately after execution of step S301; The execution of step S301 and step S302 also can be interval, namely step S302 is performed again every for some time after execution of step S301, certainly, have a rest here in process, gas barrier 12 can be kept to be in exhaust condition always, the gaseous product produced in step S301 all can be discharged reaction chamber like this, and then the cleaning efficiency of step S302 can be improved.
Above-described embodiment one and embodiment two mainly describe the situation that using plasma (the first cleaning of plasma and/or the second cleaning plasma) removes the settling (carbonaceous organic material and/or metal and compound) thereof of reaction chamber inside in detail, in fact, the mode of the settling generation thermal response of clean air and reaction chamber inside can also be adopted in the embodiment of the present invention to remove this settling.
Embodiment three
The embodiment of the present invention three provides a kind of method of In-Situ Cleaning MOCVD reaction chamber, the method of the method and the embodiment of the present invention one is similar, different, adopt the mode of clean air and settling generation thermal response to remove the settling of reaction chamber inside in the embodiment of the present invention three.For simplicity, only introduce the difference with the embodiment of the present invention one in the embodiment of the present invention three, those skilled in the art easily obtain the other guide of the embodiment of the present invention three from the associated description of the embodiment of the present invention one, do not repeat them here.
Step S401: pass into the first clean air to reaction chamber 10 inside, maintain the temperature of reaction chamber 10 inside between 200 DEG C to 500 DEG C, and the pressure of reaction chamber 10 inside is remained on first time period in the first predetermined pressure range with remove reaction chamber 10 inside carbonaceous organic material and by part metals and converting compounds thereof for metal oxide;
The first clean air in the embodiment of the present invention two can comprise the first oxygen-containing gas, and wherein the first oxygen-containing gas can be O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O; Preferably, the first oxygen-containing gas in the embodiment of the present invention selects the gas with strong oxidizing property, as O
3, H
2o
2deng.
Particularly, can remain in the first predetermined pressure range (as 0.1 ~ 10 holder) by making the inwall of reaction chamber 10 and/or the mode of base 13 and/or spray header 11 heating the pressure of reaction chamber 10 inside, control the temperature of reaction chamber 10 inside to remain between 200 DEG C to 500 DEG C (as 200 DEG C, 300 DEG C, 500 DEG C etc.), react to make the carbonaceous organic material in the first clean air and settling.Adopt the method, the mode of a step can be adopted to remove carbonaceous organic material in the settling of reaction chamber 10 inside completely.
It should be noted that, in the embodiment of the present invention three, any one or two steps in following step S401-A1 and step S401-A2 can be performed with alternative steps S401:
Step S401-A1: pass into the first clean air to reaction chamber 10 inside, and by Internal reforming at reaction chamber 10 for the first clean air be the first cleaning plasma;
Step S401-A2: in reaction chamber 10 outside, described first clean air is converted into the first cleaning plasma, and the first cleaning plasma is passed into the inside of reaction chamber 10;
Wherein, the first clean air in step S401-A1 and step S401-A2 can have identical implication with the first clean air in step S401.
In addition, step S401-A1 and step S401-A2 can also be performed, the carrying out reacted with further expedite clean-up while execution step S401.
Step S402: pass into the second clean air to reaction chamber 10 inside, maintain the temperature of reaction chamber 10 between 200 DEG C to 500 DEG C, and the pressure of reaction chamber 10 inside to be remained in the second predetermined pressure range for the second time period to remove the metal oxide of reaction chamber 10 inside;
After the second clean air passes into reaction chamber 10 inside, the pressure of reaction chamber 10 inside can be maintained in the example of 0.1Torr ~ 10Torr(as the second predetermined pressure range) between more than 3 minutes (as 5 ~ 30 minutes), fully there is the metal halide that thermal response forms gaseous state to make in the second clean air and settling residual metal and compound thereof and discharge reaction chamber by gas barrier.
The first clean air in the embodiment of the present invention three and the first clean air in the embodiment of the present invention one have the second clean air in identical implication, the embodiment of the present invention three and the second clean air in the embodiment of the present invention one has identical implication.
It should be noted that, in the embodiment of the present invention three, the execution of step S401 and step S402 can continuous print, namely performs step S402 immediately after execution of step S401; The execution of step S401 and step S402 also can be interval, namely step S402 is performed again every for some time after execution of step S401, certainly, have a rest here in process, gas barrier 12 can be kept to be in exhaust condition always, the gaseous product produced in step S401 all can be discharged reaction chamber like this, and then the cleaning efficiency of step S402 can be improved.
It should be noted that; parameter (as pressure, time, temperature etc.), gaseous fraction, content etc. in the embodiment of the present invention one and/or embodiment two describe the scheme be equally applicable in the embodiment of the present invention three; for simplicity; in this no longer repeated description; but the scheme in the embodiment of the present invention three still can combine with the corresponding contents in the embodiment of the present invention one and/or embodiment two thus obtain concrete implementation by those of ordinary skill in the art, and these implementations are still within protection scope of the present invention.
Visible, the settling generation thermal response of clean air and reaction chamber inside can be adopted in the embodiment of the present invention thus this settling is removed, also can first clean air be converted into cleaning plasma and then adopt the settling of this cleaning plasma and reaction chamber inside to react thus this settling is removed; Wherein, this cleaning plasma can be formed in the outside of reaction chamber, also can be formed in the inside of reaction chamber (can be formed in the reaction zone of reaction chamber inside, also can be formed in the inner region except reaction zone of reaction chamber).Adopt the scheme in the above embodiment of the present invention, the mode of a step can be adopted to remove the carbonaceous organic material of reaction chamber inside and metal and compound thereof completely.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. a method for In-Situ Cleaning MOCVD reaction chamber, is characterized in that, described method comprises:
Perform step (a):
Pass into the first clean air to described reaction chamber inside, and the temperature maintaining described reaction chamber inside is between 200 DEG C to 500 DEG C;
And the pressure of described reaction chamber inside is remained on first time period in the first predetermined pressure range with remove completely described reaction chamber inside carbonaceous organic material and by the metal of described reaction chamber inside and converting compounds thereof for metal oxide; Wherein, described first clean air comprises the first oxygen-containing gas, and described first clean air also comprises the second halogen-containing gas, and described second halogen-containing gas comprises HCl, BCl
3, Cl
2, H
2/ Cl
2mixed gas, one or several combination in HBr; Described first oxygen-containing gas comprises O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O;
Perform step (b):
Pass into the second clean air to described reaction chamber inside, and the temperature maintaining described reaction chamber inside is between 200 DEG C to 500 DEG C;
And the pressure of described reaction chamber inside to be remained in the second predetermined pressure range for the second time period to remove the metal oxide of described reaction chamber inside completely; Wherein said second clean air comprises the first halogen-containing gas, and described first halogen-containing gas comprises HCl, BCl3, BCl/O
2mixed gas, H
2/ Cl
2mixed gas, Cl
2, one or several combination in HBr.
2. method according to claim 1, is characterized in that, described first clean air also comprises Ar; And/or described second clean air also comprises Ar.
3. method according to claim 1, is characterized in that, described in described first clean air, the molar fraction of the first oxygen-containing gas is greater than the molar fraction of described second halogen-containing gas.
4. method according to claim 1, is characterized in that, described second clean air also comprises the second oxygen-containing gas, and described second oxygen-containing gas comprises O
2, O
3, CO
2, H
2o
2, N
2one or several combination in O, CO.
5. method according to claim 4, is characterized in that, described in described second clean air, the molar fraction of the first halogen-containing gas is greater than the molar fraction of described second oxygen-containing gas.
6. the method according to any one of claim 1-5, is characterized in that, described first time period is greater than 5 minutes, and described second time period is greater than 3 minutes.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210364958.XA CN102899636B (en) | 2012-09-26 | 2012-09-26 | A kind of method of In-Situ Cleaning MOCVD reaction chamber |
| KR1020130112051A KR20140040643A (en) | 2012-09-26 | 2013-09-17 | Method for in situ cleaning of mocvd reaction chamber |
| US14/032,138 US20140083453A1 (en) | 2012-09-26 | 2013-09-19 | Method for in situ cleaning of mocvd reaction chamber |
| TW102134864A TWI535884B (en) | 2012-09-26 | 2013-09-26 | Method of cleaning MOCVD reaction chamber in situ |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210364958.XA CN102899636B (en) | 2012-09-26 | 2012-09-26 | A kind of method of In-Situ Cleaning MOCVD reaction chamber |
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| Publication Number | Publication Date |
|---|---|
| CN102899636A CN102899636A (en) | 2013-01-30 |
| CN102899636B true CN102899636B (en) | 2015-12-09 |
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| CN201210364958.XA Active CN102899636B (en) | 2012-09-26 | 2012-09-26 | A kind of method of In-Situ Cleaning MOCVD reaction chamber |
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| Country | Link |
|---|---|
| US (1) | US20140083453A1 (en) |
| KR (1) | KR20140040643A (en) |
| CN (1) | CN102899636B (en) |
| TW (1) | TWI535884B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352205B (en) * | 2013-05-31 | 2015-11-25 | 上海华力微电子有限公司 | The cleaning method of CVD (Chemical Vapor Deposition) chamber |
| US10265742B2 (en) * | 2013-11-25 | 2019-04-23 | Applied Materials, Inc. | Method for in-situ chamber clean using carbon monoxide (CO) gas utlized in an etch processing chamber |
| KR102357845B1 (en) * | 2013-12-02 | 2022-01-28 | 어플라이드 머티어리얼스, 인코포레이티드 | Methods and apparatus for in-situ cleaning of a process chamber |
| CN105986244B (en) * | 2015-02-16 | 2019-01-01 | 中微半导体设备(上海)有限公司 | A kind of chemical vapor deposition unit and its clean method |
| CN106191809B (en) * | 2015-02-16 | 2018-12-25 | 中微半导体设备(上海)有限公司 | A kind of chemical vapor deposition unit and its clean method |
| CN105177533B (en) * | 2015-09-07 | 2017-11-03 | 哈尔滨工业大学 | A kind of method of utilization plasma situ cleaning MWCVD nacelles |
| CN106540927A (en) * | 2015-09-23 | 2017-03-29 | 北京北方微电子基地设备工艺研究中心有限责任公司 | The cleaning method of reaction chamber |
| CN106609358B (en) * | 2015-10-27 | 2018-12-18 | 中微半导体设备(上海)有限公司 | A kind of chemical vapor deposition unit and its clean method |
| US10453925B2 (en) | 2016-01-29 | 2019-10-22 | Taiwan Semiconductor Manufacturing Co., Ltd. | Epitaxial growth methods and structures thereof |
| CN107039485A (en) | 2016-02-03 | 2017-08-11 | 昆山工研院新型平板显示技术中心有限公司 | A kind of pixel arrangement structure, evaporation mask plate and special-shaped display screen body |
| CN106702348B (en) * | 2016-12-29 | 2019-06-18 | 圆融光电科技股份有限公司 | The method for eliminating water oxygen molecular impurity in MOCVD device reaction chamber |
| GB2559615A (en) * | 2017-02-13 | 2018-08-15 | Edwards S R O | Cleaning method |
| JP7094131B2 (en) * | 2018-04-03 | 2022-07-01 | 東京エレクトロン株式会社 | Cleaning method |
| JP7241627B2 (en) * | 2019-07-05 | 2023-03-17 | 東京エレクトロン株式会社 | Cleaning method and plasma processing apparatus |
| CN113564562A (en) * | 2021-07-08 | 2021-10-29 | 哈工大机器人(中山)无人装备与人工智能研究院 | MPCVD cavity cleaning method |
| CN114086154A (en) * | 2021-11-24 | 2022-02-25 | 苏州昶明微电子科技合伙企业(有限合伙) | Vacuum chamber online cleaning method |
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| CN100410421C (en) * | 2001-05-04 | 2008-08-13 | 拉姆研究公司 | Duo-step plasma cleaning of chamber residues |
| JP2008288281A (en) * | 2007-05-15 | 2008-11-27 | Hitachi Kokusai Electric Inc | Manufacturing method of semiconductor device and substrate treatment apparatus |
| JP2009123795A (en) * | 2007-11-13 | 2009-06-04 | Hitachi Kokusai Electric Inc | Manufacturing method of semiconductor device and substrate treatment apparatus |
| WO2011031521A2 (en) * | 2009-08-27 | 2011-03-17 | Applied Materials, Inc. | Method of decontamination of process chamber after in-situ chamber clean |
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2012
- 2012-09-26 CN CN201210364958.XA patent/CN102899636B/en active Active
-
2013
- 2013-09-17 KR KR1020130112051A patent/KR20140040643A/en not_active Application Discontinuation
- 2013-09-19 US US14/032,138 patent/US20140083453A1/en not_active Abandoned
- 2013-09-26 TW TW102134864A patent/TWI535884B/en active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011097A (en) * | 2010-12-17 | 2011-04-13 | 中微半导体设备(上海)有限公司 | Method for eliminating sediment residues of compounds of elements in groups III and V |
| CN102586753A (en) * | 2012-03-21 | 2012-07-18 | 中微半导体设备(上海)有限公司 | Method for cleaning metal organic chemical vapor deposition (MOCVD) device |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI535884B (en) | 2016-06-01 |
| US20140083453A1 (en) | 2014-03-27 |
| CN102899636A (en) | 2013-01-30 |
| KR20140040643A (en) | 2014-04-03 |
| TW201430163A (en) | 2014-08-01 |
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